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Hydrochloric Acid → 1,6-Dihydro-4-hydroxy-1-methyl-2-methoxy-6-oxo-pyrimidine

HRID 261788
ノート
印刷プレビュー

反応式

HRID 261788 の反応式
[OH:1][C:2]1[N:3]=[C:4](SC)[N:5]([CH3:9])[C:6](=[O:8])[CH:7]=1.[CH3:12][OH:13].Cl>CCOCC>[OH:1][C:2]1[N:3]=[C:4]([O:13][CH3:12])[N:5]([CH3:9])[C:6](=[O:8])[CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 1354085986-Hydroxy-1-methyl-2-(methylsulfanyl)pyrimidin-4(1h)-one

生成物 1

HCID 1358484661,6-Dihydro-4-hydroxy-1-methyl-2-methoxy-6-oxo-pyrimidine収率 40%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

A mixture of 172 g (1 mol) of 1,6-dihydro-4-hydroxy-1-methyl-2-methylthio-6-oxo-pyrimidine, 700 ml of methanol and 5 ml of a solution of hydrogen chloride in ether was boiled for 10 days under reflux. The reaction mixture was then filtered while still hot and the filtrate is evaporated in vacuo. The residue was triturated with ether and the crystalline product was filtered off. In this way, 71 g (40% of theory) of 1,6-dihydro-4-hydroxy-1-methyl-2-methoxy-6-oxo-pyrimidine were obtained in the form of colorless crystals of melting point 170°-171° C. ##STR11##

後処理

  1. temperatureunder reflux
  2. filtrationThe reaction mixture was then filtered while still hot and the filtrate
  3. customis evaporated in vacuo
  4. customThe residue was triturated with ether
  5. filtrationthe crystalline product was filtered off

出典と根拠

ORDレコード
ord-be41bb75b42b464f9fa7713bb4e877ed
出典データセット
uspto-grants-1979_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04152426

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート